#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:46:14 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262573 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/19/7241921.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7241921
loop_
_publ_author_name
'Jung, Mi-Hee'
_publ_section_title
;
 Exploration of two-dimensional perovskites incorporating methylammonium
 for high performance solar cells
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1181
_journal_page_last               1200
_journal_paper_doi               10.1039/D0CE01469A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_sum            'C2 H8 I3 N Pb'
_chemical_formula_weight         633.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-11-16 deposited with the CCDC.	2020-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1520(16)
_cell_length_b                   8.7470(18)
_cell_length_c                   15.148(3)
_cell_measurement_reflns_used    15449
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.749
_cell_measurement_theta_min      0.401
_cell_volume                     1080.1(4)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1475
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10824
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.099
_diffrn_reflns_theta_min         2.838
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    23.904
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.899
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_refine_diff_density_max         2.685
_refine_diff_density_min         -2.605
_refine_diff_density_rms         0.377
_refine_ls_extinction_coef       0.026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         2070
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.252
_refine_ls_shift/su_mean         0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1184P)²+1.6134P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1872
_reflns_number_total             2070
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01469a2.cif
_cod_data_source_block           EAPbI3_1_a
_cod_depositor_comments
'Adding full bibliography for 7241916--7241921.cif.'
_cod_database_code               7241921
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.51162(5) 0.250000 0.75280(2) 0.0507(2) Uani 1 2 d S T P . .
C1 C 0.382(4) -0.250000 0.630(2) 0.183(16) Uani 1 2 d DS T P . .
H1A H 0.313746 -0.200562 0.672943 0.275 Uiso 0.5 1 calc R U P . .
H1AB H 0.483793 -0.195996 0.624686 0.275 Uiso 0.5 1 calc R U P . .
H1AC H 0.402522 -0.353442 0.647749 0.275 Uiso 0.5 1 calc R U P . .
I002 I 0.74231(8) 0.50272(6) 0.67183(6) 0.0726(3) Uani 1 1 d . . . . .
C2 C 0.298(3) -0.250000 0.545(2) 0.26(3) Uani 1 2 d DS T P . .
H2A H 0.325881 -0.340361 0.510643 0.310 Uiso 0.5 1 calc R U P . .
H2AB H 0.325881 -0.159639 0.510643 0.310 Uiso 0.5 1 calc R U P . .
I003 I 0.28997(15) 0.250000 0.58396(5) 0.0838(4) Uani 1 2 d S T P . .
N3 N 0.124(2) -0.250000 0.5700(19) 0.180(14) Uani 1 2 d DS T P . .
H3A H 0.112162 -0.297275 0.621612 0.270 Uiso 0.5 1 calc R U P . .
H3B H 0.065742 -0.298652 0.528980 0.270 Uiso 0.5 1 calc R U P . .
H3C H 0.088619 -0.154073 0.574631 0.270 Uiso 0.5 1 calc R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4371 1.8409 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.4194 10.2008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I003 Pb01 I002 91.52(3) . . ?
I003 Pb01 I002 91.52(2) . 7_565 ?
I002 Pb01 I002 89.11(3) . 7_565 ?
I003 Pb01 I002 84.22(2) . 4_456 ?
I002 Pb01 I002 175.04(2) . 4_456 ?
I002 Pb01 I002 93.52(3) 7_565 4_456 ?
I003 Pb01 I002 84.22(2) . 6_557 ?
I002 Pb01 I002 93.52(3) . 6_557 ?
I002 Pb01 I002 175.04(2) 7_565 6_557 ?
I002 Pb01 I002 83.55(3) 4_456 6_557 ?
I003 Pb01 I003 172.70(4) . 6_657 ?
I002 Pb01 I003 83.30(2) . 6_657 ?
I002 Pb01 I003 83.30(2) 7_565 6_657 ?
I002 Pb01 I003 101.17(2) 4_456 6_657 ?
I002 Pb01 I003 101.17(2) 6_557 6_657 ?
C2 C1 H1A 118.3 . . ?
C2 C1 H1AB 118.4 . . ?
H1A C1 H1AB 99.4 . . ?
C2 C1 H1AC 117.9 . . ?
H1A C1 H1AC 99.5 . . ?
H1AB C1 H1AC 99.7 . . ?
Pb01 I002 Pb01 78.086(19) . 6_657 ?
C1 C2 N3 103(2) . . ?
C1 C2 H2A 111.1 . . ?
N3 C2 H2A 111.3 . . ?
C1 C2 H2AB 111.1 . . ?
N3 C2 H2AB 111.3 . . ?
H2A C2 H2AB 109.2 . . ?
Pb01 I003 Pb01 77.78(2) . 6_557 ?
C2 N3 H3A 109.5 . . ?
C2 N3 H3B 109.4 . . ?
H3A N3 H3B 109.5 . . ?
C2 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C2 N3 H3A 110(6) . 7 ?
H3A N3 H3A 55.4 . 7 ?
H3B N3 H3A 141.0 . 7 ?
H3C N3 H3A 57.1 . 7 ?
C2 N3 H3B 109(6) . 7 ?
H3A N3 H3B 141.0 . 7 ?
H3B N3 H3B 57.1 . 7 ?
H3C N3 H3B 55.4 . 7 ?
H3A N3 H3B 109.5 7 7 ?
C2 N3 H3C 109.47(12) . 7 ?
H3A N3 H3C 57.1 . 7 ?
H3B N3 H3C 55.4 . 7 ?
H3C N3 H3C 141.0 . 7 ?
H3A N3 H3C 109.5 7 7 ?
H3B N3 H3C 109.5 7 7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 I003 3.1315(10) . ?
Pb01 I002 3.1508(8) . ?
Pb01 I002 3.1508(7) 7_565 ?
Pb01 I002 3.3181(8) 4_456 ?
Pb01 I002 3.3181(8) 6_557 ?
Pb01 I003 3.3562(11) 6_657 ?
C1 C2 1.457(10) . ?
C1 H1A 1.0449 . ?
C1 H1AB 1.0448 . ?
C1 H1AC 1.0418 . ?
C2 N3 1.472(10) . ?
C2 H2A 0.9700 . ?
C2 H2AB 0.9700 . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3A 0.9(2) 7 ?
N3 H3B 0.9(2) 7 ?
N3 H3C 0.890(5) 7 ?
